CN109400937A - The preparation method of highly conductive gas sensor material based on nanofiber - Google Patents
The preparation method of highly conductive gas sensor material based on nanofiber Download PDFInfo
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Abstract
The preparation method of the invention discloses a kind of highly conductive gas sensor material based on nanofiber, belongs to sensing material technical field.The preparation method includes poly-dopamine, polyethyleneimine being successively respectively adopted modified basis material is made to basis material progress surface modification, substrate material surface growth in situ metal organic framework nanofiber after modification again, and handled through high temperature cabonization, highly conductive gas sensor material is prepared.The gas sensor material is on the basis of holding metal organic framework nanofiber good three-dimensional net structure, it is carbonized with poly-dopamine coating high-temp as conductive layer, guarantees that material obtained has the gas sensing advantage of highly sensitive selectivity height and fast response time.
Description
Technical field
The present invention relates to gas sensors, belong to sensing material technical field, are based on nanofiber more particularly to one kind
Highly conductive gas sensor material preparation method.
Background technique
Electrochemical gas sensor is that one kind can convert corresponding electric signal for information such as the concentration of gas, compositions,
And realize the material devices sensed to gas with various molecule, have in the fields such as environmental monitoring and scientific research and widely answers
With.
Sensor may be implemented to object gas by the regulation of aperture structure and surface chemical structure to material at present
Stable, sensitive and highly selective sensing detection.The oxide of the metals such as zinc, tin is shown because of its unique surface chemistry
Excellent gas sensing performance, uses as the key material of gas sensor always for a long time.However, metal oxide
Usually do not have porous structure, the absorption of material for gaseous prepared therefrom and concentration effect are not high enough, and it is sensitive to reduce sensing
Property and selectivity.
On the other hand, metal-organic framework materials are to be formed by rigid chain organic ligand and metal salt by chemical bonds
The material with porous structure, pore-size is adjustable, and large specific surface area, porosity are high, is conducive to gas molecule in material
In infiltration, diffusion, play the role of good preenrichment to light concentration gas, and selectivity suction can be carried out to specific molecular
It is attached, and then improve sensitivity and selectivity that sensor detects light concentration gas.Therefore, metal organic framework material in recent years
Material has been increasingly being used for gas sensing and detection.However, metal-organic framework materials are usually graininess, especially
When it is having a size of nanoscale, particle is easy to reunite, not easy to be processed, it is difficult to it is high effectively to play metal-organic framework materials
The advantageous feature of specific surface area.In addition, its response speed is also difficult to reach the level of INVENTIONConventional metal-oxide at present.
In conclusion metal-organic framework materials can be had both to the Gao Ling of gas sensing by design on material structure
It the advantages of sensitivity and selectivity, the response speed of metal oxide and easy processing, that is, has a very important significance, it may have compared with
Big challenge.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of highly conductive gas sensor material based on nanofiber
Preparation method.The preparation method by obtaining poly-dopamine coating in substrate material surface in-situ polymerization, then with after PEI crosslinking,
Metal organic framework nanofiber be ensure that in the growth in situ of substrate material surface, the gas sensor material pair being prepared
Gas sensing has the advantage that highly sensitive, selectivity is high and corresponding speed is fast.
To achieve the above object, the system of the invention discloses a kind of highly conductive gas sensor material based on nanofiber
Preparation Method, it includes that poly-dopamine, polyethyleneimine is successively respectively adopted to be made modified to basis material progress surface modification
Basis material, then in the modified substrate material surface growth in situ metal organic framework nanofiber, and through high temperature
Highly conductive gas sensor material is prepared in carbonization treatment.
Further, as follows to the process that basis material progress surface is modified:
After taking the cleaned processing of basis material, drying, places it in processing in dopamine solution and obtain poly-dopamine surface
The modified basis material in poly-dopamine surface is placed on through deionized water repeated flushing poly- by modified basis material
It is handled in aziridine solution, takes out, after deionized water repeated flushing, be dried to obtain modified basis material, be sealed.
Preferably, the dopamine solution is to take dopamine to be dissolved in the Tri-HCl buffer that pH value is 8.5 to be arranged to
To (Tri(Hydroxymethyl) Amino Methane Hydrochloride buffer solution).
Optimal, the concentration of the dopamine solution is 20g/L.
Optimal, the concentration of the polyethylenimine solution is 1g/L.
Preferably, it is 37 DEG C that the temperature of solution, which all controls, when surface is modified.
Further, the fibre diameter of the metal organic framework nanofiber is 50nm~1 μm, and fibre length is 5 μm
~100 μm.
Further, the metal organic framework nanofiber is prepared by lanthanide metal salt and organic ligand.
Further, the lanthanide metal salt includes a kind of in Eu (europium), Gd (gadolinium), Tb (terbium), Sm (samarium) or Yb (ytterbium)
The mixture of the compound of the compound of element or two kinds and two or more elements composition.
Further, the organic ligand includes trimesic acid, citric acid, nitrilotriacetic acid, 2, and 2 ';6,2 "-connection three
At least one of pyridine or diethylenetriamine.
Further, in the process of the modified substrate material surface growth in situ metal organic framework nanofiber
It is as follows:
The modified basis material is placed in lanthanide series metal salting liquid and handles a period of time, is set again after taking out washing
In organic ligand solution, room temperature or temperature reaction, then washed repeatedly using ethyl alcohol and deionized water, it is impregnated in ethyl alcohol, take out,
The basis material of dry surface in situ growth metal organic framework nanofiber.
Preferably, the washing is also to be washed using deionized water.
Preferably, the room temperature reaction is 24~72h of isothermal reaction at 20~30 DEG C.
Preferably, the temperature reaction is to be to slowly warm up to 90~160 DEG C with the heating rate of 10 DEG C/min, isothermal reaction
6~for 24 hours.
Preferably, the drying is under vacuum condition, and controlled at 100 DEG C, optimal drying time is 3h.
Preferably, the lanthanide series metal salting liquid be in Eu, Gd, Tb, Sm or Yb a kind of compound of element or two kinds and
The mixture of the compound composition of two or more elements is placed in be configured by the in the mixed solvent that organic solvent and water form
Solution.Preferably, the volume ratio of the organic solvent and water is 1:23.
Preferably, the organic solvent is at least one of ethyl alcohol, the tert-butyl alcohol or isopropanol.
Preferably, the concentration of the lanthanide series metal salting liquid is 0.02~0.1mol/L.
Preferably, the organic ligand solution be trimesic acid, citric acid, nitrilotriacetic acid, 2,2 ';6,2 "-connection three
At least one of pyridine or diethylenetriamine are placed in the solution configured by the in the mixed solvent that organic solvent and water form.
Preferably, the volume ratio of the organic solvent and water is 2:1.
Preferably, the organic solvent is at least one of ethyl alcohol, the tert-butyl alcohol or isopropanol.
Preferably, the concentration of the organic ligand solution is 0.08~0.4mol/L.
Further, the high temperature cabonization processing is graphene sheet layer structure to make poly-dopamine carbonization pyrolysis, wherein stone
Black alkene lamellar structure can form high connductivity layer.
Further, the condition of the high temperature cabonization processing is as follows:
800 DEG C~1200 DEG C are raised to from room temperature with 20 DEG C~50 DEG C of heating rate in a nitrogen atmosphere, constant temperature is kept
30min~60min.
Further, described matrix material is polymer nanofiber self-supported membrane, polymer nanofiber/nonwoven is applied with
One of layer composite membrane, interdigital electrode, metal nethike embrane or inorganic non-metallic nethike embrane.
Preferably, the polymer nanofiber self-supported membrane is that polymer nanofiber suspension is coated in nonwoven fabric base
On material, removes and obtain after dry.
Preferably, the polymer nanofiber/non-woven cloth coating composite membrane is the coating of polymer nanofiber suspension
On non-woven fabrics base material, obtained after dry.Preferably, polymer nanofiber suspension is applied using high pressure draught forming technique
It overlays on non-woven fabrics base material.
Optimal, the polymer nanofiber suspension is that the polymer nano being prepared mutually is separated using melt blending
Rice fiber disperses to be formed in a solvent.
Optimal, the polymer nanofiber is ethylene-vinyl alcohol copolymer, polyethylene terephthalate, gathers
Ethylene octene is total at least one of elastomer, nylon 6, polypropylene, polystyrene, polyvinyl chloride or Kynoar.
Preferably, the interdigital electrode are as follows: ceramics, PET, aluminium oxide, aluminum-nitride-based gold electrode;Preferably, wherein pitching
Refer to that electrode wires spacing is 3 μm~10 μm, 0.3 μm~1 μm of interdigital electrode metal layer thickness.
Preferably, the metal nethike embrane are as follows: using the nethike embrane that stainless steel, aluminium, copper are done as material, preferably, wherein nethike embrane
Mesh length be 20 μm~100 μm, metal nethike embrane with a thickness of 10 μm~200 μm.
Preferably, the inorganic non-metallic nethike embrane are as follows: with ceramics, aluminium oxide, aluminium nitride, carbon fiber is the net that material is done
Film, preferably, wherein the mesh size of nethike embrane be 3 μm~50 μm, inorganic non-metallic nethike embrane with a thickness of 7 μm~200 μm.
The invention also discloses the gas sensor materials being prepared using above-mentioned preparation method, it includes matrix material
Material is aggregated in the poly-dopamine coating of substrate material surface, and the polyethyleneimine with poly-dopamine coating crosslinking, also wraps
Include the metal organic framework nanofiber in substrate material surface growth in situ, wherein poly-dopamine coating is obtained through high-temperature process
Conductive layer, and metal organic framework nanofiber forms three-dimensional net structure in space, can give full play to the gas of material
Sensing capabilities.
The beneficial effects are mainly reflected as follows as follows:
The preparation method that the present invention designs realizes effective knot of metal organic framework nanofiber Yu poly-dopamine coating
It closes, on the basis of holding metal organic framework nanofiber good three-dimensional net structure, the carbonization of poly-dopamine coating high-temp is
Conductive layer guarantees that the material of preparation has the gas sensing advantage of highly sensitive selectivity height and fast response time.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the highly conductive gas sensor material of the present invention;
Wherein, each label is as follows in Fig. 1:
Metal organic framework layers of nanofibers 1, graphene conductive layer 2, basis material 3.
Specific embodiment
In order to better explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but
The contents of the present invention are not limited solely to following embodiment.
Embodiment 1
The NaOH solution of the ethylene-vinyl alcohol copolymer nanofiber 1mol/L of preparation will be mutually separated by melt blending
After being ultrasonically treated 30min, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 10mol/L.
The ethylene-vinyl alcohol copolymer nanofiber that cleaning treatment is crossed is put into DA solution and is vibrated for 24 hours at 37 DEG C,
Deionized water repeated flushing is used after fully reacting, obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution (aqueous solution, similarly hereinafter) of 1g/L, 37
3h is vibrated at DEG C and is rinsed to obtain the modified substrate in the surface PEI-PDA with deionized water.
By the modified substrate infiltration in the surface PEI-PDA in the six nitric hydrate europium solution that concentration is 0.02mol/L
1h is handled, is rinsed 3 times after taking-up with deionized water, then places it in the trimesic acid solution for being 0.08mol/L containing concentration
Reaction kettle in, at 100 DEG C react 48h (solvent of organic ligand and metal salt solution is the mixed solvent of alcohol water, preferably
Alcohol is ethyl alcohol) obtain membrane material.It takes out and is cleaned repeatedly 3 times with deionized water, ethyl alcohol, the membrane material that will be obtained after fully reacting
It is placed in ethyl alcohol and impregnates 12h, take out vacuum drying 3h and obtain the composite base material that surface growth has metal organic framework fiber.In nitrogen
Controlled at 800 DEG C under gas shielded, there is the composite base material of metal organic framework fiber to carry out at carbonization surface growth
Reason, to obtain based on the highly conductive gas sensing device material of nanofiber.
Wherein, in conjunction with Fig. 1 it is found that gas sensor material obtained above includes basis material 3, it is aggregated in basis material
The poly-dopamine coating on 3 surfaces, and the polyethyleneimine with poly-dopamine coating crosslinking, and poly-dopamine coating high-temp carbon
It is melted into graphene conductive layer 2, by the crosslinked action of polyethyleneimine, in substrate material surface also growth in situ porous porous gold
Belong to oxide nanofiber and obtain metal organic framework layers of nanofibers 1, to form three-dimensional net structure in space, has this
The material of structure can give full play to gas sensing performance.
Embodiment 2
The NaOH of the polyethylene terephthalate nanofiber 1mol/L of preparation will be mutually separated by melt blending
After solution is ultrasonically treated 30min, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 11mol/L.
The polyethylene terephthalate nanofiber that cleaning treatment is crossed is put into DA solution and is vibrated at 37 DEG C
For 24 hours, deionized water repeated flushing is used after fully reacting, obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the gadolinium nitrate hexahydrate solution that concentration is 0.03mol/L
2h is handled, is rinsed 3 times after taking-up with deionized water, then is placed it in containing the anti-of the citric acid solution that concentration is 0.08mol/L
It answers in kettle, reacts for 24 hours that (solvent of organic ligand and metal salt solution is the mixed solvent of alcohol water, and preferred alcohols are at 100 DEG C
Isopropanol) obtain membrane material.It takes out after fully reacting and is cleaned repeatedly 3 times with deionized water, ethyl alcohol, obtained membrane material is set
12h is impregnated in ethyl alcohol, is taken out vacuum drying 3h and is obtained the composite base material that surface growth has metal organic framework fiber.In nitrogen
Controlled at 850 DEG C under protection, there is the composite base material of metal organic framework fiber to carry out carbonization treatment surface growth,
To obtain based on the highly conductive gas sensing device material of nanofiber.
Embodiment 3
The NaOH for the polyethylene octene elastomer nanofiber 1mol/L for mutually separating preparation by melt blending is molten
After liquid is ultrasonically treated 30min, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 12mol/L.
The polyethylene octene elastomer nanofiber that cleaning treatment is crossed is put into DA solution and is vibrated at 37 DEG C
For 24 hours, deionized water repeated flushing is used after fully reacting, obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the six nitric hydrate terbium solution that concentration is 0.05mol/L
1h is handled, is rinsed 4 times after taking-up with deionized water, then places it in the nitrilotriacetic acid solution for being 0.12mol/L containing concentration
Reaction kettle in, at 110 DEG C react 72h (solvent of organic ligand and metal salt solution is the mixed solvent of alcohol water, preferably
Alcohol is ethyl alcohol) obtain membrane material.It takes out and is cleaned repeatedly 3 times with deionized water, ethyl alcohol, the membrane material that will be obtained after fully reacting
It is placed in ethyl alcohol and impregnates 12h, take out vacuum drying 3h and obtain the composite base material that surface growth has metal organic framework fiber.In nitrogen
Controlled at 900 DEG C under gas shielded, there is the composite base material of metal organic framework fiber to carry out at carbonization surface growth
Reason, to obtain based on the highly conductive gas sensing device material of nanofiber.
Embodiment 4
The NaOH solution ultrasonic treatment of the nylon 6/nanometer fiber 1mol/L of preparation will be mutually separated by melt blending
After 30min, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 13mol/L.
The nylon 6/nanometer fiber that cleaning treatment is crossed is put into DA solution and is vibrated for 24 hours at 37 DEG C, is used after fully reacting
Deionized water repeated flushing obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the six nitric hydrate samarium solution that concentration is 0.05mol/L
1h is handled, is rinsed 5 times after taking-up with deionized water, then is placed it in containing 2,2 ' that concentration is 0.14mol/L;6,2 "-connection three
In the reaction kettle of pyridine solution, react for 24 hours that (solvent of organic ligand and metal salt solution is that the mixing of alcohol water is molten at 90 DEG C
Agent, preferred alcohols are ethyl alcohol) obtain membrane material.It takes out after fully reacting and is cleaned repeatedly 3 times with deionized water, ethyl alcohol, will be obtained
Membrane material be placed in ethyl alcohol and impregnate 12h, taking out vacuum drying 3h and obtaining surface growth has the compound of metal organic framework fiber
Substrate.Under nitrogen protection controlled at 950 DEG C, to the surface growth have the composite base material of metal organic framework fiber into
Row carbonization treatment, to obtain based on the highly conductive gas sensing device material of nanofiber.
Embodiment 5
The NaOH solution ultrasonic treatment of the polypropylene nano fiber 1mol/L of preparation will be mutually separated by melt blending
After 30min, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 14mol/L.
The polypropylene nano fiber that cleaning treatment is crossed is put into DA solution and is vibrated for 24 hours at 37 DEG C, after fully reacting
With deionized water repeated flushing, the modified substrate in the surface PDA is obtained.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the six nitric hydrate ytterbium solution that concentration is 0.06mol/L
5h is handled, is rinsed 5 times after taking-up with deionized water, then places it in the diethylenetriamine solution for being 0.16mol/L containing concentration
Reaction kettle in, at 90 DEG C react 6h (solvent of organic ligand and metal salt solution is the mixed solvent of alcohol water, preferred alcohols
For ethyl alcohol) obtain membrane material.It takes out after fully reacting and is cleaned repeatedly 3 times with deionized water, ethyl alcohol, obtained membrane material is set
12h is impregnated in ethyl alcohol, is taken out vacuum drying 3h and is obtained the composite base material that surface growth has metal organic framework fiber.In nitrogen
Controlled at 1000 DEG C under protection, there is the composite base material of metal organic framework fiber to carry out at carbonization surface growth
Reason, to obtain based on the highly conductive gas sensing device material of nanofiber.
Embodiment 6
The polystyrene nano fiber that preparation is mutually separated by the melt blending NaOH solution of 1mol/L is ultrasonically treated
After 30min, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 10mol/L.
The ethylene-vinyl alcohol copolymer nanofiber that cleaning treatment is crossed is put into DA solution and is vibrated for 24 hours at 37 DEG C,
Deionized water repeated flushing is used after fully reacting, obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the six nitric hydrate ruthenium solutions that concentration is 0.07mol/L
1h is handled, is rinsed 3 times after taking-up with deionized water, then places it in the trimesic acid solution for being 0.18mol/L containing concentration
Reaction kettle in, at 20 DEG C react 72h (solvent of organic ligand and metal salt solution is the mixed solvent of alcohol water, preferably
Alcohol is ethyl alcohol) obtain membrane material.It takes out and is cleaned repeatedly 3 times with deionized water, ethyl alcohol, the membrane material that will be obtained after fully reacting
It is placed in ethyl alcohol and impregnates 12h, take out vacuum drying 3h and obtain the composite base material that surface growth has metal organic framework fiber.In nitrogen
Controlled at 1050 DEG C under gas shielded, there is the composite base material of metal organic framework fiber to carry out at carbonization surface growth
Reason, to obtain based on the highly conductive gas sensing device material of nanofiber.
Embodiment 7
The NaOH solution ultrasonic treatment of the polyvinyl chloride nano fiber 1mol/L of preparation will be mutually separated by melt blending
After 30min, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 11mol/L.
The ethylene-vinyl alcohol copolymer nanofiber that cleaning treatment is crossed is put into DA solution and is vibrated for 24 hours at 37 DEG C,
Deionized water repeated flushing is used after fully reacting, obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the six nitric hydrate europium solution that concentration is 0.08mol/L
1h is handled, is rinsed 3 times after taking-up with deionized water, then places it in the trimesic acid solution for being 0.10mol/L containing concentration
With concentration be 0.10mol/L nitrilotriacetic acid solution mixed solution reaction kettle in, at 90 DEG C react 6h (organic ligand with
And the solvent of metal salt solution is the mixed solvent of alcohol water, and preferred alcohols are ethyl alcohol) obtain membrane material.It is taken out simultaneously after fully reacting
It is cleaned repeatedly 3 times with deionized water, ethyl alcohol, obtained membrane material is placed in ethyl alcohol and impregnates 12h, taken out vacuum drying 3h and obtain
Surface grows the composite base material for having metal organic framework fiber.Under nitrogen protection controlled at 1100 DEG C, to the surface
Growth has the composite base material of metal organic framework fiber to carry out carbonization treatment, to obtain passing based on the highly conductive gas of nanofiber
Inductor component material.
Embodiment 8
The NaOH solution of the ethylene-vinyl alcohol copolymer nanofiber 1mol/L of preparation will be mutually separated by melt blending
After being ultrasonically treated 30min, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 12mol/L.
The ethylene-vinyl alcohol copolymer nanofiber that cleaning treatment is crossed is put into DA solution and is vibrated for 24 hours at 37 DEG C,
Deionized water repeated flushing is used after fully reacting, obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the gadolinium nitrate hexahydrate solution that concentration is 0.09mol/L
1h is handled, is rinsed 3 times after taking-up with deionized water, then places it in the trimesic acid solution for being 0.11mol/L containing concentration
It is the 2,2 ' of 0.11mol/L with concentration;6,2 " it is (organic that 72h is reacted in the reaction kettle of-ter cycloheptapyridine mixed solution, at 100 DEG C
The solvent of ligand and metal salt solution is the mixed solvent of alcohol water, and preferred alcohols are ethyl alcohol) obtain membrane material.After fully reacting
It takes out and is cleaned repeatedly 3 times with deionized water, ethyl alcohol, obtained membrane material is placed in ethyl alcohol and impregnates 12h, take out vacuum drying
3h obtains the composite base material that surface growth has metal organic framework fiber.Under nitrogen protection controlled at 1150 DEG C, to institute
Stating surface growth has the composite base material of metal organic framework fiber to carry out carbonization treatment, to obtain highly conductive based on nanofiber
Gas sensing device material.
Embodiment 9
The polymer nanofiber self-supported membrane (ethylene-vinyl alcohol copolymer) that preparation is mutually separated by melt blending is used
After the NaOH solution ultrasonic treatment 30min of 1mol/L, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 13mol/L.
The ethylene-vinyl alcohol copolymer nanofiber that cleaning treatment is crossed is put into DA solution and is vibrated for 24 hours at 37 DEG C,
Deionized water repeated flushing is used after fully reacting, obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the six nitric hydrate europium solution that concentration is 0.10mol/L
2h is handled, is rinsed 4 times after taking-up with deionized water, then places it in the trimesic acid solution for being 0.13mol/L containing concentration
In the reaction kettle of the mixed solution for the diethylenetriamine solution that concentration is 0.11mol/L, (organic ligand for 24 hours is reacted at 40 DEG C
And the solvent of metal salt solution is the mixed solvent of alcohol water, and preferred alcohols are ethyl alcohol) obtain membrane material.It is taken out after fully reacting
And cleaned repeatedly 3 times with deionized water, ethyl alcohol, obtained membrane material is placed in ethyl alcohol and impregnates 12h, vacuum drying 3h is taken out and obtains
The composite base material for having metal organic framework fiber is grown to surface.Under nitrogen protection controlled at 1200 DEG C, to the table
The composite base material with metal organic framework fiber of looking unfamiliar carries out carbonization treatment, to obtain based on the highly conductive gas of nanofiber
Senser element material.
Embodiment 10
The interdigital electrode (ceramics) that preparation is mutually separated by the melt blending NaOH solution of 1mol/L is ultrasonically treated
After 30min, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 14mol/L.
The ethylene-vinyl alcohol copolymer nanofiber that cleaning treatment is crossed is put into DA solution and is vibrated for 24 hours at 37 DEG C,
Deionized water repeated flushing is used after fully reacting, obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the six nitric hydrate europium solution that concentration is 0.26mol/L
2h is handled, is rinsed 4 times after taking-up with deionized water, then places it in the trimesic acid solution for being 0.02mol/L containing concentration
And concentration is the 2,2 ' of 0.03mol/L;6,2 " in the reaction kettle of-ter cycloheptapyridine solution mixed solution, 5h is reacted at 100 DEG C
(solvent of organic ligand and metal salt solution is the mixed solvent of alcohol water, and preferred alcohols are ethyl alcohol) obtains membrane material.Reaction
It takes out after completely and is cleaned repeatedly 3 times with deionized water, ethyl alcohol, obtained membrane material is placed in ethyl alcohol and impregnates 12h, take out true
The dry 3h of sky obtains the composite base material that surface growth has metal organic framework fiber.Under nitrogen protection controlled at 800 DEG C,
There is the composite base material of metal organic framework fiber to carry out carbonization treatment surface growth, to obtain high based on nanofiber
Gaseous conductor senser element material.
Embodiment 11
After the NaOH solution for mutually separating the metal nethike embrane 1mol/L of preparation by melt blending is ultrasonically treated 30min,
It is successively washed with deionized water, ethyl alcohol, deionized water again then dry.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 10mol/L.
The ethylene-vinyl alcohol copolymer nanofiber that cleaning treatment is crossed is put into DA solution and is vibrated for 24 hours at 37 DEG C,
Deionized water repeated flushing is used after fully reacting, obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the six nitric hydrate europium solution that concentration is 0.28mol/L
Handle 2h, after taking-up with deionized water rinse 4 times, then place it in containing concentration be 0.04mol/L citric acid solution with it is dense
Degree be 0.03mol/L diethylenetriamine solution mixed solution reaction kettle in, at 30 DEG C react 48h (organic ligand and
The solvent of metal salt solution is the mixed solvent of alcohol water, and preferred alcohols are ethyl alcohol) obtain membrane material.It takes out and is used in combination after fully reacting
Deionized water, ethyl alcohol clean 3 times repeatedly, and obtained membrane material is placed in ethyl alcohol and impregnates 12h, take out vacuum drying 3h and obtain table
It looks unfamiliar the composite base material with metal organic framework fiber.Under nitrogen protection controlled at 900 DEG C, the surface is grown
There is the composite base material of metal organic framework fiber to carry out carbonization treatment, to obtain based on the highly conductive gas sensor of nanofiber
Part material.
Embodiment 12
The NaOH solution ultrasonic treatment of the inorganic non-metallic nethike embrane 1mol/L of preparation will be mutually separated by melt blending
After 30min, then then drying is successively washed with deionized water, ethyl alcohol, deionized water.
The pH value that dopamine (DA) is dissolved in 100mL is by dopamine (DA) solution for configuring 20g/L in configuration process
In 8.5 Tri(Hydroxymethyl) Amino Methane Hydrochloride (Tri-HCl) buffer, the concentration of Tri-HCl buffer is 13mol/L.
The ethylene-vinyl alcohol copolymer nanofiber that cleaning treatment is crossed is put into DA solution and is vibrated for 24 hours at 37 DEG C,
Deionized water repeated flushing is used after fully reacting, obtains the modified substrate in the surface PDA.
The modified substrate in the surface PDA is placed in polyethyleneimine (PEI) solution of 1g/L, 3h is vibrated at 37 DEG C and is used in combination
Deionized water rinses to obtain the modified substrate in the surface PEI-PDA.
By the modified substrate infiltration in the surface PEI-PDA in the six nitric hydrate ruthenium solutions that concentration is 0.30mol/L
2h is handled, is rinsed 4 times after taking-up with deionized water, then places it in the nitrilotriacetic acid solution for being 0.03mol/L containing concentration
The 2,2' for being 0.03mol/L with concentration;6,2 " it is (organic that 10h is reacted in the reaction kettle of-ter cycloheptapyridine mixed solution, at 120 DEG C
The solvent of ligand and metal salt solution is the mixed solvent of alcohol water, and preferred alcohols are ethyl alcohol) obtain membrane material.After fully reacting
It takes out and is cleaned repeatedly 3 times with deionized water, ethyl alcohol, obtained membrane material is placed in ethyl alcohol and impregnates 12h, take out vacuum drying
3h obtains the composite base material that surface growth has metal organic framework fiber.Under nitrogen protection controlled at 1000 DEG C, to institute
Stating surface growth has the composite base material of metal organic framework fiber to carry out carbonization treatment, to obtain highly conductive based on nanofiber
Gas sensing device material.
The preparation method that the present invention designs is by obtaining poly-dopamine coating in substrate material surface in-situ polymerization, the poly- DOPA
Amine coating and PEI crosslinking after, ensure that metal organic framework nanofiber substrate material surface can growth in situ, be prepared into
To gas sensor have the advantage that highly sensitive, selectivity is high and corresponding speed is fast to gas sensing.
Above embodiments are only best citing, rather than a limitation of the embodiments of the present invention.Except above-described embodiment
Outside, there are also other embodiments by the present invention.All technical solutions formed using equivalent substitution or equivalent transformation, all fall within the present invention
It is required that protection scope.
Claims (10)
1. a kind of preparation method of the highly conductive gas sensor material based on nanofiber, it is characterised in that: it includes successively
Poly-dopamine, polyethyleneimine is respectively adopted, modified basis material is made to basis material progress surface modification, then in institute
Modified substrate material surface growth in situ metal organic framework nanofiber is stated, and is handled through high temperature cabonization, is prepared
Highly conductive gas sensor material.
2. the preparation method of the highly conductive gas sensor material based on nanofiber, feature exist according to claim 1
In: the fibre diameter of the metal organic framework nanofiber is 50nm~1 μm, and fibre length is 5 μm~100 μm.
3. the preparation method of the highly conductive gas sensor material based on nanofiber, feature exist according to claim 2
In: the metal organic framework nanofiber is prepared by lanthanide metal salt and organic ligand.
4. the preparation method of the highly conductive gas sensor material based on nanofiber, feature exist according to claim 3
In: the lanthanide metal salt includes a kind of inorganic compound or at least two elements of element composition in Eu, Gd, Tb, Sm or Yb
The mixture of the inorganic compound of composition.
5. the preparation method of the highly conductive gas sensor material based on nanofiber, feature exist according to claim 3
In: the organic ligand includes trimesic acid, citric acid, nitrilotriacetic acid, 2,2 ';6,2 "-ter cycloheptapyridine or divinyl three
At least one of amine.
6. the preparation method of the highly conductive gas sensor material according to claims 1 to 5 based on nanofiber, feature
It is: as follows in the process of the modified substrate material surface growth in situ metal organic framework nanofiber:
The modified basis material is placed in lanthanide series metal salting liquid and is handled, it is molten to be placed in organic ligand again after taking-up washing
In liquid, room temperature or temperature reaction, then washed using ethyl alcohol and deionized water, it is impregnated in ethyl alcohol, takes out, dries to obtain surface in situ life
The basis material of long metal organic framework nanofiber.
7. the preparation method of the highly conductive gas sensor material based on nanofiber, feature exist according to claim 1
In: the high temperature cabonization processing is graphene sheet layer structure to make poly-dopamine carbonization pyrolysis.
8. the preparation method of the highly conductive gas sensor material based on nanofiber, feature exist according to claim 7
In: the condition of the high temperature cabonization processing is as follows:
Be raised to 800 DEG C~1200 DEG C from room temperature with 20 DEG C~50 DEG C of heating rate in a nitrogen atmosphere, constant temperature keep 30min~
60min。
9. the preparation method of the highly conductive gas sensor material based on nanofiber, feature exist according to claim 1
In: described matrix material be polymer nanofiber self-supported membrane, it is polymer nanofiber/non-woven cloth coating composite membrane, interdigital
One of electrode, metal nethike embrane or inorganic non-metallic nethike embrane.
10. the preparation method of the highly conductive gas sensor material based on nanofiber, feature exist according to claim 1
In: it is as follows that the modified process in surface is carried out to basis material:
After taking the cleaned processing of basis material, drying, places it in processing in dopamine solution and obtain the modification of poly-dopamine surface
The modified basis material in poly-dopamine surface is placed on polyethyleneimine through deionized water flushing by basis material afterwards
It is handled in solution, takes out, after deionized water flushing, be dried to obtain modified basis material, be sealed.
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